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Separation preparing method for aloe-emodin and parietic acid

A technology of aloe-emodin and rhein, which is applied in the purification/separation/stabilization of organic compounds, organic chemical methods, chemical instruments and methods, etc., and can solve the problems of low purity and low recovery rate.

Inactive Publication Date: 2004-04-21
北京天纯维通生物技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing literature reports adopt column chromatography and high performance liquid chromatography to separate, but the purity is not high, and the recovery rate is very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Select n-hexane-ethanol-water to separate and purify the aloe-emodin and rhein in the rhubarb crude extract obtained by Soxhlet extraction on a semi-preparative countercurrent chromatograph, and first configure the above-mentioned solvent components according to the volume ratio of 5:1:5 In a separatory funnel, shake well and let stand to separate layers. After equilibrating for a period of time, the upper phase and the lower phase were separated, and the upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder, FC-95 automatic distillation copy collector. Weigh 400 mg rhubarb crude extract sample and dissolve in 20 mL mobile phase for use. Before sample injection, fill the entire column wit...

Embodiment 2

[0010] Chloroform-methanol-water was used to separate and purify the aloe-emodin and rhein in the crude rhubarb extract by using a semi-preparative countercurrent chromatograph. Firstly, the above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 4:3:2, shaken up, and allowed to stand for stratification. After equilibrating for a period of time, the upper phase and the lower phase were separated, and the upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. A semi-preparative high-speed countercurrent chromatograph is used, equipped with NS-1007 pump, 20mL injection valve, polytetrafluoroethylene column with a column volume of 240mL, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder, FC-95 automatic distillation copy collector. Weigh 100mg of rhubarb crude extract sample and dissolve it in 20mL mobile phase for use. Before sample injection, fill the entire column with stati...

Embodiment 3

[0012] The petroleum ether-propyl acetate-acetonitrile-water component was used to separate and purify the aloe-emodin and rhein in the rhubarb crude extract after column chromatography on an analytical countercurrent chromatograph. Firstly, the above-mentioned solvent components were arranged in a separatory funnel according to the volume ratio of 9:1:5:5, shaken up and left to stand to separate layers. After equilibrating for a period of time, the upper phase and the lower phase were separated, and the upper phase was used as the stationary phase, and the lower phase was used as the mobile phase. Analytical high-speed countercurrent chromatograph equipped with NS-1007 pump, 1mL injection valve, polytetrafluoroethylene column with a column volume of 40mL, 8823A-UV ultraviolet detector, Yokogawa 3057 portable recorder, FC-95 automatic fractionation collector. Weigh 15 mg of rhubarb crude extract and dissolve it in 1 mL of mobile phase for use. Before sample injection, fill t...

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PUM

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Abstract

A process for separating aloe-emodin and rhein from rhubarb and purifying them by high-speed counter-current chromatography features that its used solvent is the combination of some of petroleum ether, heptane, hexane, pentane, chloroform, dichloromethane, CCL4, acetonitrile, methanol, ethanol, acetone, ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate and water. Its avdantage is high purity up to 98% or more.

Description

technical field [0001] The invention relates to a method for preparing and separating high-purity monomer aloe-emodin (Aloe-emodin) and rhein (rhein) from rhubarb by adopting high-speed countercurrent chromatography. Background technique [0002] Rhubarb is one of the four famous medicinal materials of traditional Chinese medicine. Its pharmacological uses are very extensive. The main functions are: breaking stasis and promoting blood circulation, attacking diarrhea heat, antibacterial and anti-inflammatory, protecting liver and diuresis, mediating immunity, delaying aging, reducing fat and losing weight, anti-tumor, hemostasis and pain relief Wait. Moreover, it is also used in the preparation of fructose, beverages, spices, brewing and industrial dyes and other industries. Rhubarb is bitter and cold in nature and has the effects of conquering stagnant stagnation, purging fire and cooling blood, promoting blood circulation and removing blood stasis, promoting gallbladder an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B63/00C07C50/34C07C66/02
Inventor 魏芸张天佑
Owner 北京天纯维通生物技术有限公司
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